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CN106007723A - Making method of SiC ceramic green body - Google Patents

Making method of SiC ceramic green body Download PDF

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CN106007723A
CN106007723A CN201610343281.XA CN201610343281A CN106007723A CN 106007723 A CN106007723 A CN 106007723A CN 201610343281 A CN201610343281 A CN 201610343281A CN 106007723 A CN106007723 A CN 106007723A
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powder
sic
sintering aid
sic ceramic
ceramic green
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CN106007723B (en
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陈健
黄政仁
姚秀敏
刘学建
陈忠明
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Shanghai Institute of Ceramics of CAS
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    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00Producing shaped prefabricated articles from the material
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    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00Processes of additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
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Abstract

本发明涉及一种SiC陶瓷素坯的制备方法,包括:将SiC粉体、烧结助剂、粘结剂、溶剂经球磨混合后得到混合浆料;将所得混合浆料烘干或喷雾造粒,得到混合均匀粉体粒径在50μm‑100μm之间的SiC陶瓷粉体;利用计算机辅助设计软件构造SiC陶瓷素坯的结构模型并采用激光粉体熔融制造技术或液态光敏树脂制造技术将SiC陶瓷粉体逐层打印直至形成所述SiC陶瓷素坯,其中单层厚度为0.1‑0.2mm。本发明采用3D打印技术可以根据需求,通过计算机辅助设计制备不同结构的SiC陶瓷,该方法成型过程无需模具,对产品的复杂程度敏感度不高,具有产品开发快等一系列优点。

The invention relates to a method for preparing SiC ceramic green bodies, comprising: mixing SiC powder, sintering aids, binders, and solvents through ball milling to obtain a mixed slurry; drying or spraying the obtained mixed slurry, Obtain SiC ceramic powder with mixed uniform powder particle size between 50 μm and 100 μm; use computer-aided design software to construct the structural model of SiC ceramic green body, and use laser powder fusion manufacturing technology or liquid photosensitive resin manufacturing technology to make SiC ceramic powder The body is printed layer by layer until the SiC ceramic green body is formed, wherein the thickness of a single layer is 0.1-0.2 mm. The present invention uses 3D printing technology to prepare SiC ceramics with different structures through computer-aided design according to requirements. This method does not require molds during the forming process, is not highly sensitive to product complexity, and has a series of advantages such as fast product development.

Description

一种SiC陶瓷素坯的制造方法A kind of manufacturing method of SiC ceramic biscuit

技术领域technical field

本发明涉及一种3D打印技术制备碳化硅(SiC)陶瓷素坯的方法,属于SiC陶瓷领域。The invention relates to a method for preparing silicon carbide (SiC) ceramic blanks by 3D printing technology, belonging to the field of SiC ceramics.

背景技术Background technique

碳化硅(SiC)具有原子半径小、键长短、共价键性强等特性,因而具有优良的力学、热学、电学性能和化学稳定性,同时具有耐辐照、抗放射性、吸波等特性,是重要的核反应堆耐中子辐照材料以及吸波隐身材料,被广泛应用于精密轴承、密封件、气轮机转子、热交换器部件、原子热反应堆材料及空间光学应用材料等,并日益受到人们的重视,但是SiC陶瓷所固有的高强度、高硬度等优点同时给其成型、加工带来了很多困难.尤其是形状复杂的陶瓷部件,通常需要借助于复杂的模具来实现.而复杂模具的制作具有很高的技术难度,需要较高的制作成本和较长的制作周期,而且,模具一旦制作完成,就无法再对产品进行修改.在市场竞争日趋激烈,产品更新速度日益加快的今天,这种生产状况已经越来越不能适应现代企业生存和发展的需要。Silicon carbide (SiC) has the characteristics of small atomic radius, short bond length and strong covalent bond, so it has excellent mechanical, thermal, electrical properties and chemical stability, and has the characteristics of radiation resistance, radioactivity resistance and wave absorption. It is an important nuclear reactor neutron radiation resistant material and wave-absorbing stealth material. It is widely used in precision bearings, seals, gas turbine rotors, heat exchanger components, atomic thermal reactor materials and space optical application materials, etc., and has become increasingly popular. However, the inherent high strength and high hardness of SiC ceramics bring many difficulties to its molding and processing. Especially ceramic parts with complex shapes usually need to be realized with the help of complex molds. The complex mold Production is very technically difficult, requiring high production costs and a long production cycle. Moreover, once the mold is produced, the product cannot be modified. In today's increasingly fierce market competition and faster product updates, This kind of production situation can no longer meet the needs of the survival and development of modern enterprises.

发明内容Contents of the invention

针对上述问题,本发明的目的在于提供一种快速、精确的SiC陶瓷材料的成型方法。In view of the above problems, the object of the present invention is to provide a fast and accurate forming method of SiC ceramic material.

为此,本发明提供了一种3D打印技术制备SiC陶瓷素坯的方法,包括:For this reason, the present invention provides a kind of method for preparing SiC ceramic biscuit by 3D printing technology, comprising:

将SiC粉体、烧结助剂、粘结剂、溶剂经球磨混合后得到混合浆料;Mix SiC powder, sintering aid, binder, and solvent through ball milling to obtain a mixed slurry;

将所得混合浆料烘干或喷雾造粒,得到混合均匀粉体粒径在50μm-100μm之间的SiC陶瓷粉体;Drying or spraying granulation of the obtained mixed slurry to obtain a SiC ceramic powder with a uniform powder particle size between 50 μm and 100 μm;

利用计算机辅助设计软件构造SiC陶瓷素坯的结构模型并采用激光粉体熔融制造技术或液态光敏树脂制造技术将SiC陶瓷粉体逐层打印直至形成所述SiC陶瓷素坯,其中单层厚度为0.1-0.2mm。Use computer-aided design software to construct the structural model of SiC ceramic green body, and use laser powder fusion manufacturing technology or liquid photosensitive resin manufacturing technology to print SiC ceramic powder layer by layer until the SiC ceramic green body is formed, wherein the thickness of a single layer is 0.1 -0.2mm.

本发明采用3D打印技术可以根据需求,通过计算机辅助设计制备不同结构的SiC陶瓷,该方法成型过程无需模具,对产品的复杂程度敏感度不高,具有产品开发快等一系列优点。The present invention uses 3D printing technology to prepare SiC ceramics of different structures through computer-aided design according to requirements. This method does not require molds in the molding process, is not sensitive to product complexity, and has a series of advantages such as fast product development.

较佳地,所述烧结助剂为B-C体系的烧结助剂,其中B含量不高于SiC粉体和烧结助剂总质量的1wt%,C含量不低于SiC粉体和烧结助剂总质量的2wt%。Preferably, the sintering aid is a B-C system sintering aid, wherein the B content is not higher than 1 wt% of the total mass of SiC powder and sintering aid, and the C content is not less than the total mass of SiC powder and sintering aid 2wt%.

较佳地,所述烧结助剂为Al2O3和稀土氧化物混合物,其中稀土氧化物为Y2O3、CeO2、Er2O3中的至少一种。Preferably, the sintering aid is a mixture of Al 2 O 3 and rare earth oxides, wherein the rare earth oxide is at least one of Y 2 O 3 , CeO 2 , and Er 2 O 3 .

又,较佳地,所述烧结助剂的质量不低于SiC粉体和烧结助剂总质量的5wt%。Also, preferably, the mass of the sintering aid is not less than 5 wt% of the total mass of the SiC powder and the sintering aid.

较佳地,所述粘结剂为酚醛树脂、聚乙烯醇(PVA)、聚乙烯醇缩丁醛(PVB)、聚甲基丙烯酸甲酯(PMMA)中的至少一种。Preferably, the binder is at least one of phenolic resin, polyvinyl alcohol (PVA), polyvinyl butyral (PVB), and polymethyl methacrylate (PMMA).

又,较佳地,所述粘结剂的质量不低于SiC粉体和烧结助剂总质量的5wt%。Also, preferably, the mass of the binder is not less than 5wt% of the total mass of the SiC powder and the sintering aid.

较佳地,所述溶剂为水或无水乙醇。Preferably, the solvent is water or absolute ethanol.

较佳地,所述混合浆料的固含量为40-50wt%,优选为40-45wt%。Preferably, the solid content of the mixed slurry is 40-50wt%, preferably 40-45wt%.

较佳地,所述激光粉体熔融制造技术的参数包括:激光功率为12-15W,扫描速度为1500-3000mm/s,扫描间距为0.05-0.1mm,单层厚度为0.1-0.2mm。具体方法包括:首先,在设备工作台上铺一薄层粉末材料,高能激光在计算机控制下根据制件各层截面的参数,有选择地对粉末层进行扫描,被扫描区域的粉末材料由于融化粘结在一起,一层加工完以后,工作台下降一个层厚的高度,再进行下一层铺粉和扫描,新加工层与前一层粘结为一体,重复上述过程直至整个部件加工完成为止。Preferably, the parameters of the laser powder fusion manufacturing technology include: laser power of 12-15W, scanning speed of 1500-3000mm/s, scanning distance of 0.05-0.1mm, and single layer thickness of 0.1-0.2mm. The specific methods include: first, spread a thin layer of powder material on the equipment workbench, and the high-energy laser selectively scans the powder layer according to the parameters of the cross-section of each layer under the control of the computer. The powder material in the scanned area is melted Bonded together, after one layer is processed, the workbench is lowered by a layer thickness, and then the next layer is powdered and scanned, the new processed layer is bonded with the previous layer, and the above process is repeated until the entire part is processed until.

较佳地,所述液态光敏树脂制造技术的参数包括:光敏树脂为环氧树脂体系,含量为粉体质量的2-5wt%,激光功率为15-50MW,扫描速度为2000-4000mm/s,扫描间距为0.05-0.1mm,单层厚度为0.1-0.2mm。具体来说,液态光敏树脂制造技术为由激光器发出的紫外光,经光学系统汇集成一支细光束,该光束在计算机控制下,有选择地扫描与粉体混合的液体光敏树脂表面,利用光敏树脂遇紫外光凝固的机理。一层一层地固化光敏树脂,每固化一层后,工作台下降一精确距离,并按新一层表面几何信息使激光扫描器对粉体表面树脂进行扫描,使新一层树脂固化并粘在前一层已固化的树脂上,如此反复。直至制作生成该零件实体模型。Preferably, the parameters of the liquid photosensitive resin manufacturing technology include: the photosensitive resin is an epoxy resin system, the content is 2-5wt% of the powder mass, the laser power is 15-50MW, and the scanning speed is 2000-4000mm/s, The scanning distance is 0.05-0.1mm, and the thickness of a single layer is 0.1-0.2mm. Specifically, the liquid photosensitive resin manufacturing technology is that the ultraviolet light emitted by the laser is collected into a thin beam through the optical system. Under the control of the computer, the beam selectively scans the surface of the liquid photosensitive resin mixed with the powder. Mechanism of solidification by ultraviolet light. The photosensitive resin is cured layer by layer. After each layer is cured, the workbench is lowered by a precise distance, and the laser scanner scans the resin on the surface of the powder according to the geometric information of the new layer, so that the new layer of resin is cured and adhered. Repeat this on the previous layer of cured resin. Until the production generates the solid model of the part.

附图说明Description of drawings

图1为实施例1经喷雾造粒制备的陶瓷粉体的SEM图;Fig. 1 is the SEM figure of the ceramic powder prepared by spray granulation in embodiment 1;

图2为实施例1经计算机辅助设计获得的复杂形状的SiC陶瓷结构模型图;Fig. 2 is the SiC ceramic structure model diagram of the complicated shape that embodiment 1 obtains through computer-aided design;

图3为实施例1通过3D打印技术获得的复杂形状的SiC陶瓷素坯实物图;Fig. 3 is the physical figure of the SiC ceramic green body of complex shape obtained by 3D printing technology in embodiment 1;

图4为实施例2经喷雾造粒制备的陶瓷粉体的SEM图;Fig. 4 is the SEM figure of the ceramic powder prepared by spray granulation in embodiment 2;

图5为实施例2经计算机辅助设计获得的复杂形状的SiC陶瓷结构模型图;Fig. 5 is the SiC ceramic structure model diagram of the complicated shape that embodiment 2 obtains through computer-aided design;

图6为实施例2通过3D打印技术获得的复杂形状的SiC陶瓷素坯实物图。Fig. 6 is a physical diagram of a complex-shaped SiC ceramic green body obtained by 3D printing technology in Example 2.

具体实施方式detailed description

以下结合实施方式进一步说明本发明,应理解,下述实施方式仅用于说明本发明,而非限制本发明。The present invention will be further described below in conjunction with the embodiments. It should be understood that the following embodiments are only used to illustrate the present invention, not to limit the present invention.

本发明制备可烧结的SiC均匀混合粉体。同时通过计算机辅助技术设计不同形状的SiC陶瓷结构。然后再通过液态光敏树脂制造技术或者粉体激光熔融制造技术将制备好的SiC粉体3D打印成SiC陶瓷素坯材料。The invention prepares sinterable SiC uniformly mixed powder. At the same time, different shapes of SiC ceramic structures are designed by computer aided technology. Then, the prepared SiC powder is 3D printed into SiC ceramic green body material by liquid photosensitive resin manufacturing technology or powder laser melting manufacturing technology.

以下示例性地说明本发明利用3D打印技术制备SiC陶瓷素坯的方法。The method for preparing a SiC ceramic green body by using 3D printing technology in the present invention is exemplarily described below.

本发明以SiC粉体为原料,再加入烧结助剂、粘结剂(例如,酚醛树脂、聚乙烯醇(PVA)、聚乙烯醇缩丁醛(PVB)、聚甲基丙烯酸甲酯(PMMA)等)、溶剂(例如,水或无水乙醇)后球磨混合均匀后得到固含量为40-50wt%,优选为40-45wt%的混合浆料。其中,所述粘结剂的质量不低于SiC粉体和烧结助剂总质量的5wt%。The present invention takes SiC powder as raw material, then adds sintering aid, binding agent (for example, phenolic resin, polyvinyl alcohol (PVA), polyvinyl butyral (PVB), polymethyl methacrylate (PMMA) etc.), solvent (for example, water or absolute ethanol) and ball milling to obtain a mixed slurry with a solid content of 40-50 wt%, preferably 40-45 wt%. Wherein, the mass of the binder is not less than 5wt% of the total mass of the SiC powder and the sintering aid.

上述烧结助剂可为B-C体系的烧结助剂。其中B含量不高于SiC粉体和烧结助剂总质量的1wt%,C含量不低于SiC粉体和烧结助剂总质量的2wt%。The above-mentioned sintering aid can be a sintering aid of the B-C system. Wherein the B content is not higher than 1 wt% of the total mass of the SiC powder and the sintering aid, and the C content is not lower than 2 wt% of the total mass of the SiC powder and the sintering aid.

上述烧结助剂还可为Al2O3和稀土氧化物混合物。其中,所述稀土氧化物为Y2O3、CeO2、Er2O3中的至少一种。此时烧结助剂(Al2O3和稀土氧化物混合物)的质量不低于SiC粉体和烧结助剂总质量的5wt%。The above-mentioned sintering aid can also be a mixture of Al 2 O 3 and rare earth oxides. Wherein, the rare earth oxide is at least one of Y 2 O 3 , CeO 2 , Er 2 O 3 . At this time, the mass of the sintering aid (Al 2 O 3 and rare earth oxide mixture) is not less than 5 wt% of the total mass of the SiC powder and the sintering aid.

将固含量为40-50wt%的混合浆料直接烘干或进行喷雾造粒,得到混合均匀的SiC陶瓷粉体,粉体粒径在50μm-100μm之间,如图1或图4所示。这种球形的粒径在50μm-100μm之间的粉体流动性优异,便于铺层。The mixed slurry with a solid content of 40-50wt% is directly dried or subjected to spray granulation to obtain a uniformly mixed SiC ceramic powder with a particle size between 50 μm and 100 μm, as shown in Figure 1 or Figure 4 . This kind of spherical powder with a particle size between 50μm and 100μm has excellent fluidity and is convenient for layering.

利用计算机辅助设计软件构造SiC陶瓷素坯的结构模型,如图2或图5所示。Use computer aided design software to construct the structural model of the SiC ceramic green body, as shown in Figure 2 or Figure 5.

以混合均匀的SiC陶瓷粉体为原料,根据计算机辅助设计软件构造SiC陶瓷素坯的结构模型采用激光粉体熔融制造技术将陶瓷粉体逐层打印直至形成所述SiC陶瓷素坯。Using homogeneously mixed SiC ceramic powder as raw material, the structural model of SiC ceramic green body is constructed according to computer-aided design software, and the laser powder melting manufacturing technology is used to print the ceramic powder layer by layer until the SiC ceramic green body is formed.

上述激光粉体熔融制造技术为利用高能激光束的热效应使粉末材料软化或熔化,粘结成型一系列薄层,并逐步叠加获得三维实体部件。具体的参数包括:激光功率为12-15W,扫描速度为1500-3000mm/s,扫描间距为0.05-0.1mm。其中在打印素坯时,打印的单层厚度(或称单层层厚)可为0.1-0.2mm。The above-mentioned laser powder fusion manufacturing technology is to use the thermal effect of the high-energy laser beam to soften or melt the powder material, bond and form a series of thin layers, and gradually superimpose to obtain three-dimensional solid parts. The specific parameters include: the laser power is 12-15W, the scanning speed is 1500-3000mm/s, and the scanning distance is 0.05-0.1mm. Wherein when printing the blank, the thickness of the printed single layer (or single layer thickness) may be 0.1-0.2mm.

或者以混合均匀的SiC陶瓷粉体为原料,根据计算机辅助设计软件构造SiC陶瓷素坯的结构模型采用液态光敏树脂制造技术将陶瓷粉体逐层打印直至形成所述SiC陶瓷素坯。Alternatively, uniformly mixed SiC ceramic powder is used as a raw material, and the structural model of SiC ceramic green body is constructed according to computer-aided design software, and the ceramic powder is printed layer by layer with liquid photosensitive resin manufacturing technology until the SiC ceramic green body is formed.

上述液态光敏树脂制造技术为由激光器发出的紫外光,经光学系统汇集成一支细光束,该光束在计算机控制下,有选择地扫描与粉体混合的液体光敏树脂表面,利用光敏树脂遇紫外光凝固的机理。一层一层地固化光敏树脂,每固化一层后,工作台下降一精确距离,并按新一层表面几何信息使激光扫描器对对粉体表面树脂进行扫描,使新一层树脂固化并粘在前一层已固化的树脂上,如此反复。直至制作生成该零件实体模型。其工艺是基于液态光敏树脂的光聚合原理工作的。这种液态材料在一定波长(例如,λ=325nm)和功率(例如,P=30MW)的紫外光照射下能迅速发生光聚合反应,材料从液态转变成固态。具体的参数包括:光敏树脂为环氧树脂体系,含量为粉体质量的2-5wt%,激光功率可为15-50MW,扫描速度可为2000-4000mm/s,扫描间距可为0.05-0.1mm。其中在打印素坯时,打印的单层厚度(或称单层层厚)可为0.1-0.2mm。The above-mentioned liquid photosensitive resin manufacturing technology is that the ultraviolet light emitted by the laser is collected into a thin beam through the optical system. Under the control of the computer, the beam selectively scans the surface of the liquid photosensitive resin mixed with the powder. The mechanism of solidification. The photosensitive resin is cured layer by layer. After each layer is cured, the worktable is lowered by a precise distance, and the laser scanner scans the resin on the surface of the powder according to the geometric information of the new layer, so that the new layer of resin is cured and Stick to the previous layer of cured resin, and so on. Until the production generates the solid model of the part. Its technology is based on the principle of photopolymerization of liquid photosensitive resin. The liquid material can rapidly undergo photopolymerization under the irradiation of ultraviolet light with a certain wavelength (for example, λ=325nm) and power (for example, P=30MW), and the material changes from liquid to solid. The specific parameters include: the photosensitive resin is an epoxy resin system, the content is 2-5wt% of the powder mass, the laser power can be 15-50MW, the scanning speed can be 2000-4000mm/s, and the scanning distance can be 0.05-0.1mm . Wherein when printing the blank, the thickness of the printed single layer (or single layer thickness) may be 0.1-0.2mm.

下面进一步例举实施例以详细说明本发明。同样应理解,以下实施例只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例,即本领域技术人员可以通过本文的说明做合适的范围内选择,而并非要限定于下文示例的具体数值。Examples are given below to describe the present invention in detail. It should also be understood that the following examples are only used to further illustrate the present invention, and should not be construed as limiting the protection scope of the present invention. Some non-essential improvements and adjustments made by those skilled in the art according to the above contents of the present invention all belong to the present invention scope of protection. The specific process parameters and the like in the following examples are only examples of suitable ranges, that is, those skilled in the art can make a selection within a suitable range through the description herein, and are not limited to the specific values exemplified below.

实施例1Example 1

将SiC粉体965g、烧结助剂B4C(0.5wt%)5g、C黑(3wt%)30g,粉体共1000g,另外加入酚醛树脂100g、PMMA 100g混合,配成固含量为45wt%的浆料(溶剂为无水乙醇),以SiC球2000g为球磨介质,混合24h,喷雾造粒获得混合均匀粉体的粒径大小为60μm左右的SiC粉体,如图1所示。同时根据计算机辅助设计获得不同形状的SiC陶瓷结构,如图2所示。通过激光粉体熔融制造3D打印技术,激光功率15W,扫描速度为1500mm/s,扫描间距为0.1mm。其中单层打印的层厚为0.1mm。将粉体打印获得复杂形状的SiC陶瓷素坯,如图3所示。图3为打印的SiC热交换板素坯。965g of SiC powder, 5g of sintering aid B 4 C (0.5wt%), 30g of C black (3wt%), 1000g of powder in total, 100g of phenolic resin and 100g of PMMA were added and mixed to form a solid content of 45wt%. Slurry (the solvent is absolute ethanol), using 2000g of SiC balls as the ball milling medium, mixed for 24 hours, and spray granulated to obtain SiC powder with a uniform particle size of about 60 μm, as shown in Figure 1. At the same time, SiC ceramic structures of different shapes were obtained according to computer-aided design, as shown in Fig. 2 . The 3D printing technology is manufactured by laser powder fusion, the laser power is 15W, the scanning speed is 1500mm/s, and the scanning distance is 0.1mm. The layer thickness of single-layer printing is 0.1mm. Print the powder to obtain a SiC ceramic green body with a complex shape, as shown in Figure 3. Figure 3 is the printed SiC heat exchange plate blank.

实施例2Example 2

将SiC粉体900g、Al2O3和Y2O3(10wt%)100g共1000g粉体,另外加入PVA5g、PMMA100g混合,配成固含量为45wt%的浆料(溶剂为水),以SiC球2000g为球磨介质,混合24h,喷雾造粒获得混合均匀粉体粒径大小为50μm左右的SiC粉体(如图4所示)。同时根据计算机辅助设计获得不同形状的SiC陶瓷结构,如图5所示。通过激光粉体熔融3D打印技术,激光功率14W,扫描速度为3000mm/s,扫描间距为0.1mm。其中单层打印的层厚为0.2mm。将粉体打印获得复杂形状的SiC陶瓷素坯,如图6所示。图6为打印的SiC反射镜素坯。Mix 900g of SiC powder, 100g of Al 2 O 3 and Y 2 O 3 (10wt%), 1000g of powder in total, and add 5g of PVA and 100g of PMMA to make a slurry with a solid content of 45wt% (the solvent is water). 2000 g of balls were used as the ball milling medium, mixed for 24 hours, and spray granulated to obtain a SiC powder with a uniform powder particle size of about 50 μm (as shown in Figure 4). At the same time, SiC ceramic structures of different shapes were obtained according to computer-aided design, as shown in Fig. 5 . Through laser powder fusion 3D printing technology, the laser power is 14W, the scanning speed is 3000mm/s, and the scanning distance is 0.1mm. The layer thickness of single-layer printing is 0.2mm. The powder is printed to obtain a SiC ceramic green body with a complex shape, as shown in Figure 6. Figure 6 shows the printed SiC mirror blank.

Claims (10)

1.一种SiC陶瓷素坯的制备方法,其特征在于,包括: 1. a preparation method of SiC ceramic green body, is characterized in that, comprises: 将SiC粉体、烧结助剂、粘结剂、溶剂经球磨混合后得到混合浆料; Mix SiC powder, sintering aid, binder, and solvent through ball milling to obtain a mixed slurry; 将所得混合浆料烘干或喷雾造粒,得到混合均匀粉体粒径在50μm-100μm之间的SiC陶瓷粉体; Drying or spraying granulation of the obtained mixed slurry to obtain a SiC ceramic powder with a uniform powder particle size between 50 μm and 100 μm; 利用计算机辅助设计软件构造SiC陶瓷素坯的结构模型并采用激光粉体熔融制造技术或液态光敏树脂制造技术将SiC陶瓷粉体逐层打印直至形成所述SiC陶瓷素坯,其中单层厚度为0.1-0.2mm。 Use computer-aided design software to construct the structural model of SiC ceramic green body, and use laser powder fusion manufacturing technology or liquid photosensitive resin manufacturing technology to print SiC ceramic powder layer by layer until the SiC ceramic green body is formed, wherein the thickness of a single layer is 0.1 -0.2mm. 2.根据权利要求1所述的方法,其特征在于,所述烧结助剂为B-C体系的烧结助剂,其中B含量不高于SiC粉体和烧结助剂总质量的1wt%,C含量不低于SiC粉体和烧结助剂总质量的2wt%。 2. The method according to claim 1, wherein the sintering aid is a sintering aid of the B-C system, wherein the B content is not higher than 1wt% of the total mass of the SiC powder and the sintering aid, and the C content is not more than Less than 2wt% of the total mass of SiC powder and sintering aid. 3.根据权利要求1所述的方法,其特征在于,所述烧结助剂为Al2O3和稀土氧化物混合物,所述稀土氧化物为Y2O3、CeO2、Er2O3中的至少一种。 3. The method according to claim 1, characterized in that, the sintering aid is a mixture of Al 2 O 3 and rare earth oxides, and the rare earth oxides are Y 2 O 3 , CeO 2 , Er 2 O 3 at least one of . 4.根据权利要求3所述的方法,其特征在于,所述烧结助剂的质量不低于SiC粉体和烧结助剂总质量的5wt%。 4. The method according to claim 3, characterized in that the mass of the sintering aid is not less than 5wt% of the total mass of the SiC powder and the sintering aid. 5.根据权利要求1-4中任一项所述的方法,其特征在于,所述粘结剂为酚醛树脂、聚乙烯醇PVA、聚乙烯醇缩丁醛PVB、聚甲基丙烯酸甲酯PMMA中的至少一种。 5. according to the method described in any one in claim 1-4, it is characterized in that, described binding agent is phenolic resin, polyvinyl alcohol PVA, polyvinyl butyral PVB, polymethyl methacrylate PMMA at least one of the 6.根据权利要求5所述的方法,其特征在于,所述粘结剂的质量不低于SiC粉体和烧结助剂总质量的5wt%。 6. The method according to claim 5, characterized in that the mass of the binder is not less than 5wt% of the total mass of the SiC powder and the sintering aid. 7.根据权利要求1-6中任一项所述的方法,其特征在于,所述溶剂为水或无水乙醇。 7. The method according to any one of claims 1-6, characterized in that the solvent is water or absolute ethanol. 8.根据权利要求1-7中任一项所述的方法,其特征在于,所述混合浆料的固含量为40-50wt%,优选为40-45wt%。 8. The method according to any one of claims 1-7, characterized in that, the solid content of the mixed slurry is 40-50wt%, preferably 40-45wt%. 9.根据权利要求1-8中任一项所述的方法,其特征在于,所述激光粉体熔融制造技术的参数包括:激光功率为12-15W,扫描速度为1500-3000mm/s,扫描间距为0.05-0.1mm。 9. The method according to any one of claims 1-8, characterized in that the parameters of the laser powder fusion manufacturing technology include: laser power of 12-15W, scanning speed of 1500-3000mm/s, scanning The spacing is 0.05-0.1mm. 10.根据权利要求1-8中任一项所述的方法,其特征在于,所述液态光敏树脂制造技术的参数包括:液态光敏树脂为环氧树脂体系,含量为粉体质量的2-5wt%;激光功率为15-50MW,扫描速度为2000-4000mm/s,扫描间距为0.05-0.1mm。 10. The method according to any one of claims 1-8, characterized in that, the parameters of the liquid photosensitive resin manufacturing technology include: the liquid photosensitive resin is an epoxy resin system, and the content is 2-5wt of the powder mass %; The laser power is 15-50MW, the scanning speed is 2000-4000mm/s, and the scanning distance is 0.05-0.1mm.
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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106830901A (en) * 2017-02-20 2017-06-13 醴陵市陶瓷3D打印研究所 A kind of ceramic particle and preparation method for laser sintered ceramic 3D printing
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CN109336609A (en) * 2018-11-12 2019-02-15 中国科学院上海硅酸盐研究所 A kind of high thermal conductivity, electrical insulation liquid phase sintered silicon carbide ceramic and its SPS process preparation method
CN109592983A (en) * 2017-09-30 2019-04-09 中国科学院上海硅酸盐研究所 A kind of highly thermally conductive liquid phase sintering silicon carbide ceramic and preparation method thereof
CN110483064A (en) * 2019-08-20 2019-11-22 深圳德智达科技有限公司 A kind of 3D printing high solids content light sensitive ceramics raw material based on solid material Stereolithography, ceramic member and preparation method thereof
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CN113105244A (en) * 2021-03-26 2021-07-13 中国科学院上海硅酸盐研究所 Extrusion molding 3D printing silicon carbide ceramic and preparation method thereof
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CN115724663A (en) * 2022-11-04 2023-03-03 中国科学院上海硅酸盐研究所 full-3D printing silicon carbide ceramic optical component and preparation method thereof
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103817767A (en) * 2014-03-14 2014-05-28 邓湘凌 Method for manufacturing ceramic products with 3D printing technology
CN103936428A (en) * 2014-03-13 2014-07-23 济南大学 Preparation method of rapid molding powder material used for three dimensional printing
CN104526836A (en) * 2014-12-19 2015-04-22 南京工业大学 Solid inorganic powder 3D printing method based on selective laser melting technology
CN105198449A (en) * 2015-09-16 2015-12-30 广东工业大学 Method for preparing photocuring-formed high-density ceramic

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103936428A (en) * 2014-03-13 2014-07-23 济南大学 Preparation method of rapid molding powder material used for three dimensional printing
CN103817767A (en) * 2014-03-14 2014-05-28 邓湘凌 Method for manufacturing ceramic products with 3D printing technology
CN104526836A (en) * 2014-12-19 2015-04-22 南京工业大学 Solid inorganic powder 3D printing method based on selective laser melting technology
CN105198449A (en) * 2015-09-16 2015-12-30 广东工业大学 Method for preparing photocuring-formed high-density ceramic

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CN115724663A (en) * 2022-11-04 2023-03-03 中国科学院上海硅酸盐研究所 full-3D printing silicon carbide ceramic optical component and preparation method thereof
CN116675538A (en) * 2023-05-30 2023-09-01 中国科学院上海硅酸盐研究所 A method for preparing SiC ceramics by combined selective laser 3D printing/precursor impregnation pyrolysis/liquid phase sintering
CN116675538B (en) * 2023-05-30 2023-12-22 中国科学院上海硅酸盐研究所 Method for preparing SiC ceramic by combining selective laser 3D printing/precursor dipping pyrolysis/liquid phase sintering

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